data_GLOBAL # 1. SUBMISSION DETAILS _publ_contact_author_name 'Gleiter, Rolf' _publ_contact_author_address ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54- 8400' _publ_contact_author_fax '049 6221 54- 4205' _publ_contact_author_email 'rolf.gleiter@urz.uni-heidelberg.de' _publ_requested_journal 'Organometallics' _publ_requested_coeditor_name ? _publ_contact_letter ; paper to be submitted for publication in Organometallics ; #===END # 3. TITLE AND AUTHOR LIST _publ_section_title ; Isolation of Di(\h^2^-nitrato)(\h^4^-cyclobutadiene)cobalt(II) complexes From the oxidation of sterically hindered CpCo-stabilized cyclobutadiene complexes ; loop_ _publ_author_name _publ_author_address 'Schaefer, Carsten' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Gleiter, Rolf' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; 'Rominger, Frank' ; Organisch-Chemisches Institut Universit\"at Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #===END data_cs40 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 10a _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H38 Cl2 Co N2 O10 Si2' _chemical_formula_weight 664.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3438(2) _cell_length_b 15.0766(4) _cell_length_c 17.6375(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.5600(10) _cell_angle_gamma 90.00 _cell_volume 3006.92(12) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lamina _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7309 _exptl_absorpt_correction_T_max 0.9741 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19335 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 21.99 _reflns_number_total 3668 _reflns_number_gt 2632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+1.6293P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3668 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.57630(6) 0.67801(4) 0.33775(3) 0.0234(2) Uani 1 1 d . . . Si1 Si 0.93711(13) 0.62426(9) 0.40619(8) 0.0315(4) Uani 1 1 d . . . O1 O 0.8584(3) 0.6365(2) 0.47904(17) 0.0279(8) Uani 1 1 d . . . O2 O 0.8832(3) 0.6943(2) 0.33979(16) 0.0266(8) Uani 1 1 d . . . Si2 Si 0.30932(13) 0.86427(10) 0.38633(8) 0.0331(4) Uani 1 1 d . . . O3 O 0.4311(3) 0.9138(2) 0.36883(18) 0.0324(9) Uani 1 1 d . . . O4 O 0.3470(3) 0.7696(2) 0.42925(17) 0.0293(8) Uani 1 1 d . . . N1 N 0.3810(4) 0.6010(3) 0.3208(2) 0.0344(11) Uani 1 1 d . . . O11 O 0.4642(3) 0.5741(2) 0.36761(19) 0.0343(9) Uani 1 1 d . . . O12 O 0.4073(3) 0.6709(2) 0.28355(19) 0.0367(9) Uani 1 1 d . . . O13 O 0.2858(3) 0.5649(3) 0.3118(2) 0.0514(11) Uani 1 1 d . . . N2 N 0.6825(4) 0.6153(3) 0.2327(3) 0.0397(12) Uani 1 1 d . . . O21 O 0.6720(3) 0.5753(2) 0.2960(2) 0.0360(9) Uani 1 1 d . . . O22 O 0.6256(3) 0.6882(2) 0.22570(17) 0.0369(9) Uani 1 1 d . . . O23 O 0.7422(4) 0.5862(3) 0.1839(2) 0.0633(12) Uani 1 1 d . . . C1 C 0.6714(4) 0.7059(3) 0.4387(2) 0.0211(11) Uani 1 1 d . . . C2 C 0.7076(4) 0.7633(3) 0.3780(2) 0.0217(12) Uani 1 1 d . . . C3 C 0.5914(4) 0.8081(3) 0.3736(2) 0.0210(11) Uani 1 1 d . . . C4 C 0.5559(4) 0.7496(3) 0.4350(2) 0.0214(11) Uani 1 1 d . . . C5 C 0.7378(4) 0.6419(3) 0.4940(3) 0.0267(12) Uani 1 1 d . . . C6 C 0.8288(4) 0.7788(3) 0.3500(3) 0.0253(12) Uani 1 1 d . . . C7 C 0.5372(4) 0.8906(3) 0.3358(3) 0.0272(12) Uani 1 1 d . . . C8 C 0.4485(4) 0.7540(3) 0.4817(3) 0.0265(12) Uani 1 1 d . . . C11 C 0.6836(4) 0.5496(3) 0.4911(3) 0.0355(14) Uani 1 1 d . . . H11A H 0.6861 0.5253 0.4397 0.053 Uiso 1 1 calc R . . H11B H 0.6014 0.5530 0.5041 0.053 Uiso 1 1 calc R . . H11C H 0.7286 0.5110 0.5275 0.053 Uiso 1 1 calc R . . C12 C 0.7396(5) 0.6815(4) 0.5739(3) 0.0400(14) Uani 1 1 d . . . H12A H 0.7887 0.6445 0.6095 0.060 Uiso 1 1 calc R . . H12B H 0.6588 0.6838 0.5898 0.060 Uiso 1 1 calc R . . H12C H 0.7724 0.7416 0.5736 0.060 Uiso 1 1 calc R . . C13 C 0.8298(4) 0.8251(3) 0.2732(3) 0.0330(13) Uani 1 1 d . . . H13A H 0.9113 0.8295 0.2589 0.049 Uiso 1 1 calc R . . H13B H 0.7963 0.8848 0.2767 0.049 Uiso 1 1 calc R . . H13C H 0.7824 0.7909 0.2346 0.049 Uiso 1 1 calc R . . C14 C 0.8969(4) 0.8345(3) 0.4119(3) 0.0326(13) Uani 1 1 d . . . H14A H 0.9020 0.8019 0.4601 0.049 Uiso 1 1 calc R . . H14B H 0.8555 0.8907 0.4180 0.049 Uiso 1 1 calc R . . H14C H 0.9768 0.8464 0.3969 0.049 Uiso 1 1 calc R . . C15 C 0.5134(5) 0.8785(3) 0.2495(3) 0.0358(13) Uani 1 1 d . . . H15A H 0.4608 0.8277 0.2391 0.054 Uiso 1 1 calc R . . H15B H 0.5883 0.8681 0.2268 0.054 Uiso 1 1 calc R . . H15C H 0.4760 0.9322 0.2273 0.054 Uiso 1 1 calc R . . C16 C 0.6182(4) 0.9693(3) 0.3541(3) 0.0347(13) Uani 1 1 d . . . H16A H 0.5812 1.0233 0.3323 0.052 Uiso 1 1 calc R . . H16B H 0.6939 0.9595 0.3323 0.052 Uiso 1 1 calc R . . H16C H 0.6316 0.9759 0.4094 0.052 Uiso 1 1 calc R . . C17 C 0.4200(5) 0.6705(3) 0.5236(3) 0.0357(13) Uani 1 1 d . . . H17A H 0.3482 0.6797 0.5501 0.054 Uiso 1 1 calc R . . H17B H 0.4860 0.6559 0.5608 0.054 Uiso 1 1 calc R . . H17C H 0.4073 0.6216 0.4873 0.054 Uiso 1 1 calc R . . C18 C 0.4694(4) 0.8301(3) 0.5386(3) 0.0342(13) Uani 1 1 d . . . H18A H 0.4830 0.8852 0.5111 0.051 Uiso 1 1 calc R . . H18B H 0.5388 0.8168 0.5734 0.051 Uiso 1 1 calc R . . H18C H 0.3999 0.8369 0.5677 0.051 Uiso 1 1 calc R . . C21 C 0.9338(5) 0.5120(3) 0.3634(3) 0.0464(15) Uani 1 1 d . . . H21A H 0.9678 0.4692 0.4008 0.070 Uiso 1 1 calc R . . H21B H 0.9800 0.5120 0.3187 0.070 Uiso 1 1 calc R . . H21C H 0.8518 0.4955 0.3480 0.070 Uiso 1 1 calc R . . C31 C 1.0890(4) 0.6512(4) 0.4421(3) 0.0424(15) Uani 1 1 d . . . H31A H 1.0916 0.7117 0.4626 0.064 Uiso 1 1 calc R . . H31B H 1.1411 0.6471 0.4005 0.064 Uiso 1 1 calc R . . H31C H 1.1155 0.6093 0.4824 0.064 Uiso 1 1 calc R . . C41 C 0.2122(5) 0.8351(4) 0.3018(3) 0.0439(15) Uani 1 1 d . . . H41A H 0.1836 0.8894 0.2759 0.066 Uiso 1 1 calc R . . H41B H 0.1447 0.8008 0.3172 0.066 Uiso 1 1 calc R . . H41C H 0.2564 0.7996 0.2672 0.066 Uiso 1 1 calc R . . C51 C 0.2317(5) 0.9395(4) 0.4486(3) 0.0439(15) Uani 1 1 d . . . H51A H 0.2897 0.9761 0.4786 0.066 Uiso 1 1 calc R . . H51B H 0.1864 0.9044 0.4830 0.066 Uiso 1 1 calc R . . H51C H 0.1778 0.9780 0.4173 0.066 Uiso 1 1 calc R . . C60 C 1.0602(7) 0.6552(4) 0.1876(4) 0.069(2) Uani 1 1 d . . . H60A H 1.1313 0.6561 0.2240 0.083 Uiso 1 1 calc R . . H60B H 0.9905 0.6652 0.2168 0.083 Uiso 1 1 calc R . . Cl1 Cl 1.0700(2) 0.74109(14) 0.12343(11) 0.1071(8) Uani 1 1 d . . . Cl2 Cl 1.04845(18) 0.55291(13) 0.14582(13) 0.0927(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0306(4) 0.0239(4) 0.0155(4) -0.0018(3) 0.0003(3) -0.0004(3) Si1 0.0367(9) 0.0329(9) 0.0251(8) 0.0036(7) 0.0046(7) 0.0054(7) O1 0.024(2) 0.037(2) 0.0227(19) 0.0055(15) 0.0024(15) 0.0017(16) O2 0.033(2) 0.029(2) 0.0186(18) -0.0006(14) 0.0049(15) 0.0046(16) Si2 0.0352(9) 0.0381(9) 0.0256(8) 0.0013(7) 0.0006(7) 0.0040(7) O3 0.033(2) 0.031(2) 0.033(2) 0.0050(16) 0.0062(17) 0.0064(16) O4 0.028(2) 0.036(2) 0.0238(19) -0.0001(16) 0.0001(16) 0.0017(16) N1 0.035(3) 0.038(3) 0.031(3) -0.016(2) 0.007(2) -0.005(3) O11 0.034(2) 0.035(2) 0.034(2) -0.0023(17) 0.0016(18) -0.0035(17) O12 0.040(2) 0.041(2) 0.028(2) -0.0008(19) -0.0042(17) -0.0008(18) O13 0.032(2) 0.071(3) 0.052(3) -0.019(2) 0.006(2) -0.019(2) N2 0.041(3) 0.047(3) 0.032(3) -0.017(3) 0.007(2) -0.009(3) O21 0.045(2) 0.032(2) 0.032(2) -0.0028(18) 0.0079(18) 0.0018(17) O22 0.051(2) 0.042(2) 0.0182(19) -0.0036(16) 0.0029(17) 0.004(2) O23 0.075(3) 0.070(3) 0.048(3) -0.027(2) 0.031(2) 0.000(2) C1 0.026(3) 0.023(3) 0.014(3) -0.006(2) 0.000(2) -0.003(2) C2 0.033(3) 0.019(3) 0.012(3) -0.004(2) 0.000(2) -0.004(2) C3 0.029(3) 0.020(3) 0.014(2) -0.002(2) -0.001(2) -0.002(2) C4 0.028(3) 0.021(3) 0.015(3) -0.003(2) -0.003(2) -0.003(2) C5 0.030(3) 0.032(3) 0.018(3) 0.008(2) -0.001(2) 0.004(2) C6 0.028(3) 0.030(3) 0.018(3) 0.000(2) 0.002(2) -0.002(2) C7 0.033(3) 0.023(3) 0.026(3) 0.001(2) 0.003(2) 0.001(2) C8 0.027(3) 0.031(3) 0.021(3) -0.002(2) 0.002(2) 0.004(2) C11 0.039(3) 0.030(3) 0.038(3) 0.017(3) 0.006(3) 0.002(3) C12 0.044(3) 0.056(4) 0.020(3) 0.004(3) 0.001(3) 0.011(3) C13 0.036(3) 0.039(3) 0.025(3) 0.010(3) 0.009(2) -0.003(3) C14 0.034(3) 0.032(3) 0.032(3) 0.003(2) 0.002(3) -0.006(2) C15 0.049(4) 0.037(3) 0.021(3) 0.009(2) 0.002(3) 0.000(3) C16 0.040(3) 0.023(3) 0.042(3) 0.004(2) 0.007(3) 0.000(2) C17 0.044(3) 0.039(3) 0.026(3) 0.007(3) 0.010(3) -0.002(3) C18 0.035(3) 0.043(3) 0.025(3) -0.004(3) 0.008(2) 0.005(3) C21 0.063(4) 0.038(4) 0.039(3) 0.004(3) 0.008(3) 0.011(3) C31 0.037(3) 0.054(4) 0.037(3) 0.011(3) 0.005(3) 0.005(3) C41 0.043(4) 0.056(4) 0.032(3) 0.003(3) -0.002(3) 0.008(3) C51 0.042(4) 0.054(4) 0.035(3) 0.000(3) -0.003(3) 0.011(3) C60 0.108(6) 0.048(4) 0.052(4) -0.001(3) 0.010(4) 0.006(4) Cl1 0.171(2) 0.0864(15) 0.0601(13) 0.0196(11) -0.0145(14) -0.0173(14) Cl2 0.0913(15) 0.0703(13) 0.1163(17) -0.0390(12) 0.0071(12) 0.0006(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 2.051(4) . ? Co1 C2 2.051(4) . ? Co1 C4 2.056(4) . ? Co1 O21 2.060(3) . ? Co1 C3 2.063(4) . ? Co1 O12 2.076(3) . ? Co1 O22 2.102(3) . ? Co1 O11 2.110(3) . ? Si1 O1 1.633(3) . ? Si1 O2 1.657(3) . ? Si1 C31 1.834(5) . ? Si1 C21 1.852(5) . ? O1 C5 1.416(5) . ? O2 C6 1.433(5) . ? Si2 O3 1.622(3) . ? Si2 O4 1.656(3) . ? Si2 C41 1.835(5) . ? Si2 C51 1.851(5) . ? O3 C7 1.421(5) . ? O4 C8 1.438(5) . ? N1 O13 1.209(5) . ? N1 O11 1.270(5) . ? N1 O12 1.289(5) . ? N2 O23 1.218(5) . ? N2 O22 1.276(5) . ? N2 O21 1.282(5) . ? C1 C2 1.460(6) . ? C1 C4 1.464(6) . ? C1 C5 1.526(6) . ? C2 C3 1.478(6) . ? C2 C6 1.515(7) . ? C3 C4 1.477(6) . ? C3 C7 1.519(6) . ? C4 C8 1.525(6) . ? C5 C11 1.520(6) . ? C5 C12 1.529(7) . ? C6 C13 1.526(6) . ? C6 C14 1.536(6) . ? C7 C16 1.519(6) . ? C7 C15 1.537(6) . ? C8 C17 1.509(6) . ? C8 C18 1.530(6) . ? C60 Cl2 1.710(6) . ? C60 Cl1 1.729(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Co1 C2 41.72(17) . . ? C1 Co1 C4 41.79(17) . . ? C2 Co1 C4 60.59(18) . . ? C1 Co1 O21 102.00(16) . . ? C2 Co1 O21 101.87(16) . . ? C4 Co1 O21 142.22(16) . . ? C1 Co1 C3 60.93(17) . . ? C2 Co1 C3 42.10(17) . . ? C4 Co1 C3 42.01(17) . . ? O21 Co1 C3 142.23(17) . . ? C1 Co1 O12 144.44(16) . . ? C2 Co1 O12 144.13(16) . . ? C4 Co1 O12 104.50(16) . . ? O21 Co1 O12 106.88(13) . . ? C3 Co1 O12 103.97(16) . . ? C1 Co1 O22 129.83(16) . . ? C2 Co1 O22 92.27(16) . . ? C4 Co1 O22 143.37(16) . . ? O21 Co1 O22 62.08(14) . . ? C3 Co1 O22 101.38(16) . . ? O12 Co1 O22 82.85(14) . . ? C1 Co1 O11 102.79(16) . . ? C2 Co1 O11 144.51(16) . . ? C4 Co1 O11 94.11(15) . . ? O21 Co1 O11 82.91(13) . . ? C3 Co1 O11 131.74(16) . . ? O12 Co1 O11 61.57(14) . . ? O22 Co1 O11 119.95(13) . . ? O1 Si1 O2 106.87(17) . . ? O1 Si1 C31 105.1(2) . . ? O2 Si1 C31 112.7(2) . . ? O1 Si1 C21 115.4(2) . . ? O2 Si1 C21 107.4(2) . . ? C31 Si1 C21 109.4(3) . . ? C5 O1 Si1 138.6(3) . . ? C6 O2 Si1 128.0(3) . . ? O3 Si2 O4 106.93(17) . . ? O3 Si2 C41 114.9(2) . . ? O4 Si2 C41 106.3(2) . . ? O3 Si2 C51 106.5(2) . . ? O4 Si2 C51 112.0(2) . . ? C41 Si2 C51 110.2(2) . . ? C7 O3 Si2 136.6(3) . . ? C8 O4 Si2 126.8(3) . . ? O13 N1 O11 123.5(5) . . ? O13 N1 O12 122.8(5) . . ? O11 N1 O12 113.7(4) . . ? N1 O11 Co1 91.8(3) . . ? N1 O12 Co1 92.9(3) . . ? O23 N2 O22 123.1(5) . . ? O23 N2 O21 122.8(5) . . ? O22 N2 O21 114.1(4) . . ? N2 O21 Co1 92.6(3) . . ? N2 O22 Co1 90.9(3) . . ? C2 C1 C4 90.2(4) . . ? C2 C1 C5 133.6(4) . . ? C4 C1 C5 135.0(4) . . ? C2 C1 Co1 69.2(2) . . ? C4 C1 Co1 69.3(2) . . ? C5 C1 Co1 128.6(3) . . ? C1 C2 C3 90.4(4) . . ? C1 C2 C6 130.2(4) . . ? C3 C2 C6 137.8(4) . . ? C1 C2 Co1 69.1(2) . . ? C3 C2 Co1 69.4(2) . . ? C6 C2 Co1 129.6(3) . . ? C4 C3 C2 89.0(3) . . ? C4 C3 C7 133.3(4) . . ? C2 C3 C7 136.5(4) . . ? C4 C3 Co1 68.7(2) . . ? C2 C3 Co1 68.5(2) . . ? C7 C3 Co1 128.6(3) . . ? C1 C4 C3 90.3(4) . . ? C1 C4 C8 138.3(4) . . ? C3 C4 C8 130.3(4) . . ? C1 C4 Co1 68.9(2) . . ? C3 C4 Co1 69.3(2) . . ? C8 C4 Co1 128.4(3) . . ? O1 C5 C11 109.5(4) . . ? O1 C5 C1 110.6(4) . . ? C11 C5 C1 112.3(4) . . ? O1 C5 C12 104.6(4) . . ? C11 C5 C12 111.4(4) . . ? C1 C5 C12 108.2(4) . . ? O2 C6 C2 108.4(4) . . ? O2 C6 C13 105.2(4) . . ? C2 C6 C13 115.5(4) . . ? O2 C6 C14 112.2(4) . . ? C2 C6 C14 105.8(4) . . ? C13 C6 C14 110.0(4) . . ? O3 C7 C3 110.4(4) . . ? O3 C7 C16 103.8(4) . . ? C3 C7 C16 109.3(4) . . ? O3 C7 C15 110.3(4) . . ? C3 C7 C15 111.8(4) . . ? C16 C7 C15 111.0(4) . . ? O4 C8 C17 105.1(4) . . ? O4 C8 C4 107.1(4) . . ? C17 C8 C4 116.1(4) . . ? O4 C8 C18 112.0(4) . . ? C17 C8 C18 109.4(4) . . ? C4 C8 C18 107.3(4) . . ? Cl2 C60 Cl1 113.6(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 21.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.674 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.068 #===END